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ChemicalBook CAS DataBase List Dopamine hydrochloride
62-31-7

Dopamine hydrochloride synthesis

12synthesis methods
Dopamine hydrochloride is produced through the ring-opening reaction of piperonyl ethylamine. Piperethylamine and phenol are added to a reaction vessel and cooled down. Hydrochloric acid is slowly added while heating up the mixture to 110°C, and refluxed for 12-44 hours until the reaction reaches completion. The solution is then slightly cooled and water is added, and the mixture is stirred well and allowed to separate into layers. The upper phenolic layer is then removed, and the aqueous layer is extracted with isopropyl acetate. The extracted aqueous layer is then evaporated under reduced pressure (8.0kPa) until dry. Half the amount of ethanol and hydrochloric acid are added to the dry residue and heated to dissolve. The solution is then cooled, crystallized, and filtered. The filter cake is washed with ethanol and dried to obtain the final product, with a yield of 74%.
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Yield:62-31-7 98.6%

Reaction Conditions:

with hydrogenchloride;acetic acid in water at 160; for 6 h;Inert atmosphere;

Steps:

1.1-1.3

(1) At room temperature,Weigh 3.6320g of 3,4-dimethoxyphenethylamine (about 0.02mol, molecular weight 181.23),Place in a dry and clean three-necked round bottom flask, dissolved in 50mL of glacial acetic acid,Stir evenly to completely dissolve 3,4-dimethoxyphenethylamine;(2) Slowly add 20 mL of 37% hydrochloric acid solution (about 0.24 mol) to the reaction system,The temperature was gradually raised to 160°C, and the reaction was refluxed at 800r/min for 6 hours under nitrogen protection;(3) After the reaction is completed, concentrate under reduced pressure to remove excess acid, and add deionized water to the reaction solution.Wash the residual product on the wall, the amount is 10mL, repeat three times until there is no obvious residue on the wall,It was extracted three times with 30 mL of chloroform, the aqueous layer was taken, and the solvent was removed by rotary evaporation.Dry for 1h in a vacuum oven to obtain 3.7256g of white solid powder dopamine hydrochloride,The yield is about 98.6%.

References:

CN110981782,2020,A Location in patent:Paragraph 0031-0035

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